Gas chromatographic determination of trace carbon monoxide and carbon dioxide in sulfur hexafluoride and its application to probing potential breakdown of high-voltage circuit breaker

doi:10.3724/SP.J.1123.2019.11012

Abstract

Abstract:

A reliable gas chromatography-flame ionization detector (GC-FID) method was developed for the accurate determination of trace CO and CO₂ in high concentration of SF₆. Using a combination of dual Porapak Q chromatographic columns with valve switching, SF₆ was separated from the tested samples and blown out of the detection system, with the aim of ruling out the possibility of conversion column poisoning. Meanwhile, CO and CO₂ were on-line separated and subsequently converted to CH₄ in the presence of a nickel catalyst to increase the sensitivity for the determination of carbon-borne gases. The results showed that neither gas interfered with the determination of the other. Satisfactory linearities were achieved in the range 2-500 μL/L for both CO and CO₂, with highly accurate and reproducible determination (RSD < 2%). The developed GC-FID method is applicable to the determination of gases lodged in high-voltage circuit breakers toward the analysis of trace CO and CO₂, thus providing a tool for probing the potential breakdown of SF₆-insulated equipment.

Key words: gas chromatography (GC), carbon monoxide, carbon dioxide, sulfur hexafluoride, breakdown of circuit breaker

YANG Ren, WANG Jinxing, ZHANG Yue, WANG Qing, YUE Xuanfeng. Gas chromatographic determination of trace carbon monoxide and carbon dioxide in sulfur hexafluoride and its application to probing potential breakdown of high-voltage circuit breaker[J]. Chinese Journal of Chromatography, 2020, 38(6): 702-707.

Figures/Tables 9

Fig. 1 Column-valve GC analytical system with SF6 exclusion a. sampling step; b. injecting step. Column A: short chromatographic column (Porapak Q, 183 cm×3.8 cm (6 ft×1/8″)); column B: long chromatographic column (Porapak Q, 488 cm×3.8 cm (16 ft×1/8″)).

Fig. 2 Chromatogram of mixed gas on thermal conductivity detector (TCD) The upper and lower insets show an enlarged view of the chromatographic peaks for CO2 and CO, respectively. All the insets elsewhere in this article follow the same protocol for representation.

Fig. 3 Chromatograms of CO at various contents with CO2 at 500 μL/L

Fig. 4 Chromatograms of CO2 at various contents with CO at 500 μL/L

Table 1 Characteristics of GC method for determination of CO in the presence of varying contents of CO2

CO₂ content/(μL/L)	CO calibration equation	Correlation coefficient(r)	Linear range/(μL/L)	Total calibration equation
y: peak area of CO; x: CO content, μL/L.
20	y=7.324x-6.103	0.9999	2-500	y=7.261x-4.508
100	y=7.116x-7.253	0.9968	2-500
500	y=7.343x-1.694	0.9999	2-500

Table 2 Characteristics of GC method for determination of CO2 in the presence of varying contents of CO

CO content/(μL/L)	CO₂ calibration equation	r	Linear range/(μL/L)	Total calibration equation
y: peak area of CO₂; x: CO₂ content, μL/L.
20	y=3.104x+0.111	0.9999	2-500	y=2.994x+1.671
100	y=2.880x+1.328	0.9999	2-500
500	y=2.999x+3.574	0.9998	2-500

Fig. 5 Chromatograms for duplicate determination of 436 μL/L CO

Table 3 Standard values and measured values for control samples

Control sample	Analyte	Standard value/(μL/L)	Measured value/(μL/L)^*
* n=6, .
Sample 1	CO	15.0	14.9±0.6
	CO₂	465.0	463.7±22.3
Sample 2	CO	40.0	39.4±1.6
	CO₂	60.0	59.2±2.6

Fig. 6 Chromatograms of actual samples in circuit breakers Sample 1 and sample 2: samples from two suspicious circuit breakers; sample 3: a sample from a new circuit breaker.

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